Robot compatible crystal worksite suite

ABSTRACT

The present invention is directed to a robot compatible crystal worksite suite comprising a unique dewar, a plurality of magazines, a plurality of cryo-pins (that mount crystals to be transferred from the dewar for crystallography study) adapted to be placed into the magazines and a programmed controller to provide the operational sequence necessary to remove the frozen mounted crystals from the dewar to an instrument or a goniometer for the x-ray diffraction of the crystals.

RELATED APPLICATION

[0001] This application is based on provisional application No.60/350,920, filed Jan. 23, 2002, entitled “Crystal Carrier MagazineSystem for Use in Crystallography Applications”.

FIELD OF THE INVENTION

[0002] The present invention is directed to a suite of apparatus used inhandling crystals for x-ray crystallographic analysis. Morespecifically, the suite of apparatus includes a unique dewar, aplurality of magazines, a plurality of cryo-pins (that mount crystals tobe transferred from the dewar for crystallography study) adapted to beplaced into the magazines and a programmed controller to provide theoperational sequence necessary to remove the frozen mounted crystalsfrom the dewar to an instrument or a goniometer for the x-raydiffraction of the crystals.

BACKGROUND OF THE INVENTION

[0003] U.S. Pat. No. 6,408,047 discloses a method of performing x-raycrystallography on samples by using a robot to transfer the samples to agoniometer. This patent is incorporated herein by reference. The patentdiscloses the general system that the present invention is directed tobut does not disclose a worksite suite as disclosed herein.

[0004] U.S. Pat. No. 6,404,849 discloses a method and apparatus formounting a crystal sample for x-ray crystallographic analysis. Thispatent is incorporated herein by reference. The patent discloses thegeneral system that the present invention is directed to but does notdisclose a worksite suite as disclosed herein.

[0005] While both patents disclose the general environment of thepresent invention, the present invention is directed to a worksite suitesuitable for use when using a robot to provide the high throughput,automated crystallography methods disclosed in the patents.

SUMMARY OF THE INVENTION

[0006] The present invention is directed to a robot compatible crystalworksite suite comprising a unique dewar, a plurality of magazines, aplurality of cryo-pins (that mount crystals to be transferred from thedewar for crystallography study) adapted to be placed into the magazinesand a programmed controller to provide the operational sequencenecessary to remove the frozen mounted crystals from the dewar to aninstrument or a goniometer for the x-ray diffraction of the crystals.

BRIEF DESCRIPTION OF THE DRAWINGS

[0007]FIG. 1 is a magazine of the present invention;

[0008]FIG. 2 is an exploded view of a magazine of the present invention;

[0009]FIG. 3 is a top view of a magazine of the present invention;

[0010]FIG. 4 is a cross-sectional view of a magazine of the presentinvention along line 4-4 of FIG. 3;

[0011]FIG. 5 is a top view of a magazine tongs that is part of theworksite suite of the present invention;

[0012]FIG. 6 is a side view of the magazine tongs in FIG. 5;

[0013]FIG. 7 is a shipping rack that holds five magazines of the presentinvention;

[0014]FIG. 8 is a worksite dewar;

[0015]FIG. 9 is a partial cross-section of the dewar;

[0016]FIG. 10 is the dewar with a programmed controller;

[0017]FIG. 11 is a top view of the worksite dewar that has no magazinesinside;

[0018]FIG. 12 is a top view of the worksite dewar that has five (5)magazines inside; and

[0019]FIG. 13 is a cryo-pin tongs that removes cryo-pins from a magazinemanually and is part of the worksite suite of the present invention.

DESCRIPTION OF THE INVENTION

[0020] The central component of the suite of apparatus of the presentinvention used in handling crystals for x-ray crystallographic analysisis a multi-position magazine. The magazine is used for preciselylocating, protecting and transferring batches of crystals that requirecryogenic storage and handling. The magazine 10 is constructed from twoparts, as shown in FIG. 1 and FIG. 2. The top part 12 of magazine 10 hasa plurality of cylinders 14, specifically shown are twelve (12)cylinders; however the exact number may vary. The cylinders 14 are heldby an outer member 15 that is essentially configured as a circle. Thelower part 16 of magazine 10 has the same number of location bosses 18as cylinders 14 that are positioned to be centered in the correspondingcylinder. In each location boss 18 is a magnet 20. The strong magnets 20are held in place with epoxy to hold the cryo-pin 30, a product ofHampton Research having a ferrous base 34 (see FIG. 4), securely on thelocation bosses 18. The magnets 20 also hold the magazine 10 securely ona ferrous work surface during crystal manipulation. The upper part 12and lower part 16 of magazine 10 are held together with epoxy andpressed spring pins 24. Referring now to FIG. 3, the outer member 15conforms to surface of the cylinders 14 to provide guides 17 the grosslocation of the magazine 10. On one surface of outer member 15, a member19 is in a form to provide tabs 21 for the forceps grasping tool 40 anda slot 23 for a locking pin, described hereinafter.

[0021] The magazine 10 described in FIGS. 1-4 provides a device forprotecting and transferring twelve crystals each mounted on a cryo-pin30. The cryo-pins 30, that hold the frozen crystals, are seated in thecylinders 14 of the magazine 10 as shown in FIG. 4. The cylinders 14hold liquid nitrogen and keep the cryo-pins 30 submerged in the liquidnitrogen while the magazine 10 is transfer from one dewar to another.The cylinders 14 also protect the crystals and pins 30, which are heldto the boss 18 on the bottom part 16 of the magazine 10 by the magnets20.

[0022] The magazine 10 is handled using a grasping tool or magazinetongs 40 that utilize a “dumbbell” shaped tip 42 attached to the end offorceps 44 (FIGS. 5 and 6). The tips 42 grasp the magazine 10 viaslotted tabs 21 at the top edge of the magazine 10, as shown in FIG. 3.Since the magazine 10 is typically submerged in liquid nitrogen, themagazine tongs 40 allow the user to remove the magazine from one dewarto another. The typical dewar of the prior art has a rack with a numberof rack plates each spaced by threaded standoff members. The rack 50shown in FIG. 7 is designed to be compatible with the magazines 10 andthe suite of the present invention thus having six plates 52. The plates52 are made from martensitic stainless steel that allows the magazine 10to be held in place by the magnets 20. The threaded standoff members 54are configured to provide the spacing between plates 52 to place amagazine 10 on each plate 52 and provide a guide for the gross locationof the magazine 10 on the plate 52. A retaining bar 56 fits in slot 23of magazines 10 (FIG. 3) to securely hold the magazine 10 on the plate52. The retaining bar 56 is held in position by passing through holes inplates 52 and secured by a magnet 58. A support rod 59 is attachable tothe top plate 52 to place the five magazines into or remove themagazines from a dewar.

[0023] Reference is made to U.S. Pat. Nos. 6,408,047 and 6,494,849, bothof which are directed to providing a method of performing x-raycrystallography on samples using a robot or robotic arm. The magazines10 of the present invention are specially suited and compatible to beused in such a system. The worksite suite of the present inventionprovides for high volume of crystal samples to be tested while lesseningthe need for human intervention.

[0024] Another central component of the worksite suite of the presentinvention is the worksite dewar 60. Now referring to FIG. 8, theworksite dewar 60 provides a staging area for the crystallographysystem. The dewar 60 is placed in a mounting fixture 62 that isprecisely calibrated with the robotic arm of a robot system. Acondensation catch pan 64 is at the bottom of the dewar 60. The dewar 60has a lid 66. The dewar is a double wall flask 68 with a vacuum betweeninner wall 67 and outer wall 69. The flask 68 is capable of holdingliquid nitrogen. On the outside of the flask 68 is insulation 70. At theupper portion of the flask 68 is a rim insulator 72. A heater 75 ismounted to the rim 77 to heat the rim 77 but is insulated from the flask68. The heater 75 minimizes condensation on the rim and prevents thefreezing of any condensation that does form on the rim 77 that wouldprevent the lid 66 from opening.

[0025] Referring to FIG. 10, the worksite dewar lid actuator assembly65, is connected to a programmable controller 80 that may be separatefrom or part of the robot system. The actuator assembly 65 is comprisedof a commercial linear actuator attached to the outboard end of the lidhinge 67, beyond the lid hinge pin. The actuator assembly 65 alsoincludes micro switches which provide interlocks for both robot anddewar lid operation. When part of the robot system, the controller 80will open the lid 66 before the robotic arm enters the dewar 60 toremove or return a crystal to a magazine in the dewar 60. As shown inFIGS. 11 and 12, the worksite dewar 60 holds five magazines 10. Thefloor of flask 68 has a precision mounting plate 81 which has twentyalignment pins 82, four for each magazine for the course alignment of amagazine 10 and ten alignment pins 84 for the fine alignment of eachmagazine 10. The dewar 60 has a liquid cryogen, liquid nitrogen, inlet88 on the side of the dewar 60. As shown in FIG. 12, five magazines 10are placed in the working dewar 60, containing a total of sixty samplesof crystals to be tested by x-ray crystallography.

[0026] Pin tongs 90 are part of the suite of the present invention sincethere are occasions when the cryo-pins 30 are handled manually.

1. A magazine for storing and transferring batches of frozen mountedcrystals on cryo-pins used in crystallography applications comprising: aplurality of cylinders in which each cylinder a cryo-pin may be placed;a location boss within each of said cylinders; and a magnet centeredwith each boss for holding a cryo-pin within said cylinder.
 2. Amagazine according to claim 1 wherein an outer member surrounds saidplurality of cylinders.
 3. A magazine according to claim 1 wherein saidcylinders are configured so that said outer member is essentially acircle.
 4. A magazine according to claim 1 wherein said magazine has atop and a bottom, said bottom having said location bosses and a magneton each said boss.
 5. A magazine according to claim 1 wherein said outermember has a pair of tabs.
 6. A magazine according to claim 4 whereinsaid magazine has twelve (12) cylinders
 7. A worksite dewar for storingfrozen mounted crystals in crystallography applications held in morethan one magazine which comprises: a flask having double-walls with avacuum between the walls, said flask having a floor and wall, said floorhaving a plurality of course alignment pins that match the exteriorprofile of said magazine, and a plurality of fine alignment pins toprecisely position said magazine on said floor; and a top on said flaskwhich may be opened and closed.
 8. A worksite dewar according to claim 7which has fine alignment pins for more than four magazines.
 9. Aworksite dewar according to claim 7 which has fine alignment pins forfive (5) magazines.
 10. A worksite dewar according to claim 7 whereinsaid top is opened and closed by a programmed controller.
 11. A worksitedewar according to claim 7 which has a rim at the upper portion of saidflask and a heater in the rim of said flask.
 12. A worksite dewar forstoring frozen mounted crystals in crystallography applications held inmore than one magazine which comprises: a flask having double-walls witha vacuum between the walls, said flask having a floor and wall, and arim at the upper portion of said flask; a top on said flask which may beopened and closed; and a heater in the rim of said flask.
 13. A worksitedewar according to claim 12 wherein said top is opened and closed by aprogrammed controller.
 14. A worksite dewar according to claim 12wherein said flask holds more than four magazines.
 15. A worksite dewaraccording to claim 12 wherein said flask holds five magazines.
 16. Aworksite system used in crystallography applications comprising: adewar; a plurality of magazines which may be placed in said dewar; eachmagazine having a plurality of cylinders, each cylinder adapted to holda cryo-pin having a crystal mounted thereon; and a cryo-pin tong forremoving said cryo-pin and positioning said crystal mounted on said pinin a goniometer.
 17. A worksite system used in crystallographyapplications according to claim 16 wherein said dewar has a top that isopened and closed by a programmed controller.
 18. A worksite system usedin crystallography applications according to claim 16 wherein said dewarhas a rim at the upper portion thereof and further includes a heater insaid rim of said dewar.
 19. A worksite system used in crystallographyapplications according to claim 17 wherein said dewar has a rim at theupper portion thereof and further includes a heater in said rim of saiddewar.
 20. A worksite system used in crystallography applicationscomprising: a dewar; a programmed controller; and a top on said dewarthat is opened and closed by said programmed controller.